电感耦合等离子体原子发射光谱法测定TaNb6合金中铌和10种杂质元素

使用氢氟酸、盐酸、硝酸混合酸溶解TaNb6合金样品,选择Nb 309.418 nm、Fe 259.940 nm、Cr 267.716 nm、Ni 221.647 nm、Mn 257.610 nm、Ti 336.121 nm、Al 167.076 nm、Cu 224.700 nm、Sn 189.989 nm、Pb 261.418 nm和Zr 339.19 8 nm为分析线,在仪器最佳工作条件下,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定TaNb6合金中铌、铁、铬、镍、锰、钛、铝、铜、锡、铅和锆,从而建立了TaNb6合金中铌及10种杂质元素的测定方法。采用基体匹配法绘制校准曲线可消除基体效应的影响。各待测元素校准曲线线性回归方程的相关系数均大于0.999 5;方法中各元素的检出限为0.000 1～0.02 μg/mL。按照实验方法测定TaNb6样品中铌、铁、铬、镍、锰、钛、铝、铜、锡、铅、锆,结果的相对标准偏差(RSD,n=7)为0.021%～0.25%,与国家标准GB/T 15076—2008(钽铌合金成分测试的规定方法)测定结果相吻合。

Determination of niobium and ten impurity elements in TaNb6 alloy by inductively coupled plasma atomic emission spectrometry

The TaNb6 alloy sample was dissolved with mixed hydrofluoric acid, hydrochloric acid and nitric acid. Nb 309.418 nm, Fe 259.940 nm, Cr 267.716 nm, Ni 221.647 nm, Mn 257.610 nm, Ti 336.121 nm, Al 167.076 nm, Cu 224.700 nm, Sn 189.989 nm, Pb 261.418 nm and Zr 339.198 nm were selected as analytical lines. Under the optimal working conditions of instrument, the content of niobium, iron, chromium, nickel, manganese, titanium, aluminum, copper, tin, lead and zirconium in TaNb6 alloy was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The determination method of niobium and ten impurity elements in TaNb6 alloy was established. The calibration curves were prepared by matrix matching method to eliminate the influence of matrix effect. The linear correlation coefficients of calibration curves of testing elements were all higher than 0.999 5. The detection limits of elements in proposed method were between 0.000 1 μg/mL and 0.02 μg/mL. The content of niobium, iron, chromium, nickel, manganese, titanium, aluminum, copper, tin, lead and zirconium in TaNb6 sample was determined according to the experimental method. The relative standard deviations (RSD, n=7) were between 0.021% and 0.25%. The found results were consistent with those obtained by national standard method GB/T 15076—2008 (the specified method for the composition analysis of tantalum-niobium alloy).